A staphylococcal polysaccharide was purified by ethanol precipitation and ion-exchange and size-exclusion chromatography. It was then analyzed for monosaccharide composition by preparing the TMS derivatives of the methylglycosides followed by GC and combined GC/MS analyses. In order to prepare the sample for methylation, the sample was dissolved in DMSO and water. For glycosyl linkage analysis, the sample was methylated by the method of Ciucanu and Kerek followed by combined GC/MS. The permethylated samples were hydrolyzed using 2 M trifluoroacetic acid for 3 h at 120C. Glycosyl residues were reduced with NaBD4 and then acetylated using acetic anhydride/pyridine. GC/MS analysis was performed using a Hewlett Packard 5890 GC using a 30 m DB1 methylsilicone column coupled to a 5970 MSD. Monosaccharides were identified by their retention times in comparison to standards, and their carbohydrate character was authenticated by their mass spectra.